HPLC BTEX Separation with Carbon Phase and Gradient Elution

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Solution Overview

Problem

Conventional methods for separating and quantifying benzene, toluene, ethyl benzene, and xylenes (BTEX) are inadequate, particularly for resolving ethyl benzene and xylene isomers, which are crucial for industrial applications.

Innovation Solution

A high-performance liquid chromatography (HPLC) method using a carbon stationary phase and a mobile phase composed of organic acid in water and alcohol, with a gradient elution technique, to achieve a resolution greater than 2.0 between xylene isomer peaks.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Measurement precision

If conventional gas chromatography or Raman spectroscopy is used for BTEX analysis, then the analysis can be performed with simple equipment, but the resolution between ethyl benzene and xylene isomer peaks is insufficient

Engineering Contradiction:
Improveresolution between ethyl benzene and xylene isomer peaksVSAvoidcomplexity of chromatography system
Core Design Contradiction:
Measurement precisionVSDevice complexity

Solution Approach 1:

The patent changes the chemical composition parameters of the mobile phase by introducing formic acid (0.05-0.5 vol%) and adjusting the alcohol-to-water ratio dynamically through gradient elution. This parameter modification enables effective separation of ethyl benzene and xylene isomers that cannot be resolved by conventional methods, achieving peak resolution greater than 1.5 while maintaining system feasibility

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent implements dynamic gradient elution where the mobile phase composition changes over time during the chromatography run. The proportion of alcohol increases while water decreases in a controlled gradient, allowing optimization of separation efficiency for different compounds throughout the elution process, thereby resolving the contradiction between measurement precision and device complexity

Inventive Principle:
Principle #15Dynamics

2Measurement precision

If synthesized stationary phases are used for BTEX separation, then the separation efficiency can be improved, but the method is not commercially available for widespread application

Engineering Contradiction:
Improveseparation efficiency of BTEX compoundsVSAvoidcommercial availability of the method
Core Design Contradiction:
Measurement precisionVSEase of manufacture

Solution Approach 1:

The patent replaces expensive, custom-synthesized stationary phases with commercially available C18 reverse-phase columns that can be readily obtained and used. This substitution maintains adequate separation efficiency for BTEX compounds while dramatically improving ease of manufacture and commercial availability, allowing widespread application in research and industry

Inventive Principle:
Principle #27Cheap short-living objects (Disposable)

Solution Approach 2:

The patent compensates for the use of standard, non-specialized columns by optimizing mobile phase parameters including formic acid concentration (0.05-0.5 vol%), alcohol type and ratio, and gradient elution profiles. These parameter adjustments enable the commercially available columns to achieve separation efficiency comparable to or better than specialized synthesized phases

Inventive Principle:
Principle #35Parameter changes

3Measurement precision

If conventional liquid chromatography methods are used, then the equipment is commercially available, but the resolution between xylene isomer peaks is less than 2.0

Engineering Contradiction:
Improveresolution between xylene isomer peaksVSAvoidcomplexity of mobile phase composition and gradient elution
Core Design Contradiction:
Measurement precisionVSDevice complexity

Solution Approach 1:

The patent achieves peak resolution greater than 2.0 by precisely controlling mobile phase parameters: formic acid concentration (0.05-0.5 vol%), alcohol type (methanol, ethanol, or isopropanol), and the gradient profile. These parameter optimizations transform a standard chromatography system into one capable of high-resolution xylene isomer separation without requiring complex specialized equipment

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent introduces formic acid as an intermediary additive in the mobile phase that enhances the separation mechanism between xylene isomers. This chemical mediator improves peak resolution by modifying the interaction between analytes and the stationary phase, enabling high-resolution separation while keeping the base system relatively simple

Inventive Principle:
Principle #24Intermediary (Mediator)

Applied Scientific Principles

This section explains which scientific principles are used to turn an abstract innovation direction into a practical engineering solution.

Function Achieved in This Case

The method effectively separates and quantifies xylene isomers and ethyl benzene with a resolution greater than 2.0, enabling accurate analysis of industrial samples with minimal pre-processing.

Implementation Method 1

A stationary carbon phase... can be used

Methodology Applied
Scientific EffectAdsorption: Adsorption

Implementation Method 2

high-performance liquid chromatography for the separation of BTEX

Methodology Applied
Scientific EffectChromatography: Chromatography

Implementation Method 3

A stationary carbon phase and UV and fluorescence detectors are used

Methodology Applied
Scientific EffectFluorescence: Fluorescence

Data Source

PatentUS12298286B2Method for separation and quantitation of benzene, toluene, ethyl benzene, o-xylene, m-xylene, and p-xylene (BTEX) using high performance liquid chromatography
Publication Date: 2025.05.13 SAUDI ARABIAN OIL CO
  • US12298286B2 patent drawing
  • US12298286B2 patent drawing
  • US12298286B2 patent drawing

AI summary

Disclosed are methods and systems for quantitation of benzene, toluene, ethyl benzene, o-xylene, m-xylene, and p-xylene. High-performance liquid chromatography using a carbon stationary phase and a gradient mobile phase is performed. The carbon stationary phase can be a porous graphitic carbon stationary phase. The mobile phase includes an organic acid in water and an alcohol. The organic acid can include formic acid, and the alcohol can include methanol. The methods and systems achieve a resolution between xylene isomer peaks of greater than 2.0.